CN103730206A - Method for manufacturing transparent conducting film based on nanometer materials - Google Patents
Method for manufacturing transparent conducting film based on nanometer materials Download PDFInfo
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- CN103730206A CN103730206A CN201210385813.8A CN201210385813A CN103730206A CN 103730206 A CN103730206 A CN 103730206A CN 201210385813 A CN201210385813 A CN 201210385813A CN 103730206 A CN103730206 A CN 103730206A
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- 238000000034 method Methods 0.000 title claims abstract description 49
- 239000000463 material Substances 0.000 title claims abstract description 40
- 238000004519 manufacturing process Methods 0.000 title abstract 3
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 24
- 239000000758 substrate Substances 0.000 claims description 24
- 238000000576 coating method Methods 0.000 claims description 22
- 239000011248 coating agent Substances 0.000 claims description 19
- 239000002086 nanomaterial Substances 0.000 claims description 18
- 239000002070 nanowire Substances 0.000 claims description 15
- 229920005644 polyethylene terephthalate glycol copolymer Polymers 0.000 claims description 13
- 238000000137 annealing Methods 0.000 claims description 12
- 238000000016 photochemical curing Methods 0.000 claims description 9
- 238000000059 patterning Methods 0.000 claims description 7
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 4
- 239000002904 solvent Substances 0.000 claims description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 3
- 238000009835 boiling Methods 0.000 claims description 3
- 230000005611 electricity Effects 0.000 claims description 3
- 230000003287 optical effect Effects 0.000 claims description 3
- 229910052724 xenon Inorganic materials 0.000 claims description 3
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 claims description 3
- 238000004140 cleaning Methods 0.000 claims description 2
- 239000012459 cleaning agent Substances 0.000 claims description 2
- 239000008367 deionised water Substances 0.000 claims description 2
- 229910021641 deionized water Inorganic materials 0.000 claims description 2
- 230000010349 pulsation Effects 0.000 claims description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 2
- 229920000642 polymer Polymers 0.000 claims 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 abstract description 19
- 239000002042 Silver nanowire Substances 0.000 abstract 1
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- 238000007796 conventional method Methods 0.000 description 5
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- 238000005259 measurement Methods 0.000 description 4
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- 238000004630 atomic force microscopy Methods 0.000 description 3
- 230000000873 masking effect Effects 0.000 description 3
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 description 3
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- 238000010586 diagram Methods 0.000 description 2
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- 238000012545 processing Methods 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- 238000002834 transmittance Methods 0.000 description 2
- 230000015556 catabolic process Effects 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
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- 238000005516 engineering process Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- AMGQUBHHOARCQH-UHFFFAOYSA-N indium;oxotin Chemical compound [In].[Sn]=O AMGQUBHHOARCQH-UHFFFAOYSA-N 0.000 description 1
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Abstract
The invention relates to a method for manufacturing a transparent conducting film based on nanometer materials, in particular to silver nanowires. The method includes the single step of using a high-energy flashlamp to enable the conducting film to be annealed and patterned without postprocessing, so that the electrical conductivity is improved, basically-invisible patterns are generated on the conducting film, and the method is accordingly used for the touch panel or display manufacturing industry.
Description
Technical field
The present invention relates to preparation based on nano material, especially the method for the nesa coating of nano silver wire.The present invention includes the single step that uses high-energy flashlamp to make conducting film annealing and patterning in the situation that not needing reprocessing, to improve conductivity and the substantially sightless pattern of generation on the film of preparing industry for touch panel or display.
Background technology
The conventional method of preparing nano silver wire is by solution process, and by various coating processes, nano wire is coated on to (U.S. Patent application that publication number is 2011/0192633) on base material.The film based on nano silver wire of preparing by conventional method need to be through reprocessing or post growth annealing to obtain higher conductivity.Typical reprocessing is that film is heated to high temperature, for example, between 100-150 ℃, make it possible to remove the lip-deep non-conducting material of nano silver wire, and nano wire itself has nearer contact each other.The first problem that uses such high temperature to carry out reprocessing is possible damage film base material and conductive region.Use high-temperature post-treatment also to need time of relatively growing and higher cost.Described method also needs etch process subsequently with the step of remove portion material.High temperature is also unfavorable for any patterning of film.Conventionally need to use index-matching material, for example, when using indium tin oxide (ITO) as nesa coating, after etching-film, need to there is material that the refractive index with ITO matches so that described pattern is invisible.For the light-sensitive material of the ink that is coated with, at high temperature by thermal degradation, this destroys nano silver wire network, reduces thus the conductivity in destroyed district.If described destroyed district processes through UV light, those light-sensitive materials are further degraded, thereby conduction is poorer.On the other hand, nano silver wire is not degraded under UV exposes, and conduction is better thus.Use is conducted electricity better by restriction and the patterning of the conventional method in the poor region of conduction causes low optical property difference, can not produce sightless pattern thus in nesa coating.
In view of the above problems, need to utilize less processing step and contribute to the new method of preparing nesa coating of the patterning of film, especially prepare aspect touch panel and the figuratum display of other tools.
Summary of the invention
First aspect of the present invention relates to the method for the conducting film of preparation based on nano material, it is characterized in that by using high-energy flashlamp to adopt a step annealing and Patternized technique.Method of the present invention comprises: with at least 3 kinds of different solvent cleaned base materials; Dry described base material very first time section at the first temperature; Described base material is immersed in to the second time period in the isopropyl alcohol (IPA) of boiling; At high temperature further be dried the 3rd time period of described base material; And the ink that contains nano material is coated on base material and forms coated substrate, wherein said nano material is dissolved in organic solvent.Using described in microscopic examination after coated substrate, when described coated substrate is exposed to high-energy flashlamp lower time, by physical mask, coated substrate is being sheltered.The nano material of using in described method is nano silver wire.High-energy flashlamp used can produce the light of the high impulse of wavelength from 240nm to 1000nm.Peak power density at each impulse duration can be up to approximately 1000 times to its average power density.Conducting film prepared by method of the present invention does not need temperature-curable, but uses high-energy flashlamp during a step annealing and Patternized technique, on coated substrate, to carry out photocuring.The figuratum physical mask of tool is used to be placed between coated substrate and high-energy flashlamp, to produce pattern on conducting film during a step annealing and Patternized technique.In the situation that there is physical mask, after high-energy flashlamp exposure, on described coated substrate, form corresponding pattern.The region of those exposures conduction that becomes, and other region of being sheltered by physical mask becomes non-conductive.By a step annealing of the present invention and Patternized technique, sightless pattern substantially be can form, any heat damage or chemical depletion on etching causes in those conventional methods known in the art conducting film avoided.
Second aspect of the present invention relates to the conducting film of being prepared by method of the present invention.Conducting film of the present invention mainly comprises base material and the coating that contains a plurality of nano materials.Nano material of the present invention is nano silver wire.Nano wire of the present invention can be linear, granular, spherical or columniform.Exemplary embodiment is linear, and length is about 10-15 μ m and diameter 70nm, or draw ratio is greater than 150.More preferably, draw ratio is greater than 200.
Accompanying drawing explanation
Fig. 1: the photo of taking under light microscope, described to be cut into 12 coated substrates further to expose through high-energy flashlamp according to square net.
Fig. 2: the transmissivity of the conducting film of photocuring front and rear (%) under high-energy flashlamp.
Fig. 3: schematic diagram has been described and how to have been used high-energy flashlamp to realize a step annealing and Patternized technique: 3a (left figure) on described conducting film to have shown physical mask 302 is placed in to the example between high-energy flashlamp 301 and conducting film 303; 3b (right figure) has shown the size of the pattern 304 of preparing on conducting film by a step annealing and Patternized technique.
Fig. 4: the conductance of crossing mask border of measuring by conducting atomic force microscopy (c-AFM) changes.
Fig. 5: utilize the exposed region at conducting film of 4 point probes measurements and the sheet resistance (Rs) between non-exposed region.
Fig. 6: the SEM image (upper figure) of inclination and the SEM image (figure below) of the inclination of the nano silver wire of process photocuring under the exposure of high-energy flashlamp that do not pass through the nano silver wire of photocuring.
Embodiment
(A) the front base material of coating is clean
The preferred base material of applied nano material is PETG (PET) plate.Before coating nano material, make PET plate process cleaning procedure as herein described: (i) with cleaning agent wiping PET plate; (ii) with deionized water rinsing PET plate; (iii) with acetone rinsing PET plate; (iv) in the baking box of 70 ℃, be dried PET plate approximately 5 minutes; (v) PET plate is immersed in the isopropyl alcohol of boiling to approximately 10 minutes; (vi) PET plate is rinsed with fresh isopropyl alcohol; (vii) in the baking box of 70 ℃, be dried PET plate approximately 15 minutes.Also can be according at Adv.Mater.2011, the clean base material of the present invention of method of describing in 23,2905-2910, its disclosure is incorporated to herein by reference.
(B) preparation of coated substrate
First 10g/L nano silver wire is dissolved in the ink that contains nano silver wire with preparation in 90%v/v isopropyl alcohol/alcohol solvent.Then with apparatus for coating, the ink that contains nano silver wire is applied on PET plate.In one embodiment, described apparatus for coating is Meyer (Mayer) rod coater.The excellent size of Meyer rod can coating weight as required change.Each excellent size has the rod number of appointment, for example rod 4-20.Rod 4-20 can be used in the present invention.More specifically, use rod 4-10.In exemplary embodiment, use Meyer rod number 4 inks that coating contains nano silver wire on base material.In preferred embodiments, use Meyer at 34 ℃, described ink to be coated on base material for excellent number 4.The mobile ink that adds along with Meyer rod.In one embodiment, the mobile maintenance 120cm per minute of Meyer rod.Under syringe pump auxiliary, on base material, the speed of ink is controlled and is maintained at about under the constant rate of speed of 2-5ml/min.Actual speed rate is limited by the size of base material.Also can use other conventional coating process, for example spraying or intaglio printing, if it can produce the coated substrate with equal in quality of the present invention and quantity.After the ink that contains nano silver wire is coated on base material, then the base material of coating is dried to approximately 5 minutes in the baking box of 70 ℃.Then the coated substrate after seeing drying under light microscope.With square net, coated substrate is divided into less piece further to process (as shown in Figure 1).Described further processing includes but not limited to photocuring, annealing and/or optical masking.In exemplary, by making the coated substrate that cuts into smaller piece through the sintering system based on xenon, in single step, carry out photocuring, annealing and photoetching.
(C) step annealing and the patterning on conducting film
Use in the present invention high energy, the cooling photoflash lamp of air so that high energy pulse to be provided.In exemplary, use high energy xenon lamp so that the broad-spectrum light of 240nm to 1000nm to be provided.Preferred embodiment use 370nm to 1000nm compared with the spectrum of close limit.The average power density that is exposed to coated substrate is about 10W/cm
2.The pulsation rate of the flash of light that described photoflash lamp produces is 2 pulses approximately per second, or more specifically the pulse duration is about 0.52ms.At the peak power density of each impulse duration, be approximately 1000 times of average power density.Optionally, can use can produce identical high-caliber power density continuous light source as high-energy flashlamp of the present invention.
After high-energy flashlamp exposure, measure conducting film transmissivity and with not through the transmissivity comparison of the conducting film of exposure of flash lamp.Fig. 2 shows with there is no the conducting film of exposure and compares, and through the conducting film of the about 1-120 of exposure of flash lamp second, has identical transmittance percentage varies pattern (transmissivity measurement under wavelength 320nm transmits to the light of 800nm).Show and be exposed to the transmissivity that photoflash lamp does not affect conducting film.
Fig. 3 a and 3b are the schematic diagrames of how anneal when using high-energy flashlamp with patterning.In Fig. 3 a, physical mask 302 along light transmission route between photoflash lamp 301 and conducting film 303.Physical mask can be different on shape, pattern, size and thickness.The material of physical mask includes but not limited to glass or metal.Fig. 3 b is the example of the pattern 304 on film, and this pattern is corresponding to the corresponding pattern of physical mask.In this example, physical mask is used to masking film to produce the pattern 304 with basic identical size and dimension on conducting film under the exposure of photoflash lamp, and physical mask has two large pads by the fillet connection of a long 10mm and wide 2mm.The average power density using in this example is 10W/cm
2.Through the sheet resistor (Rs) of the conducting film of exposure of flash lamp, be about 15 Ω/.As shown in Figure 2, after exposure, the percentage transmittance of conducting film is greater than 80% (the light transmission measurement based on 400-800nm, and deduct PET base material back end).
(D) by conducting atomic force microscopy, judge that conductivity changes
In order to confirm the variation of the conductivity of conducting film, use conducting atomic force microscopy (c-AFM), and the conductivity of the electric current by c-AFM probe is changed and is shown in Fig. 4, and described c-AFM probe arrives the masking regional of conducting film from the unshielded region of conducting film through mask border.In Fig. 4, the region representation of shade is being sheltered the transition region 401 of edge, and the conductivity of film significantly changes herein.The bias voltage of 2V is applied on c-AFM probe so that electric current conducts to conducting film from probe.Result shows passes while sheltering the transition region 401 (being the shadow region in Fig. 4) on border when c-AFM probe, and the electric current of measurement significantly declines.When measure through c-AFM probe electric current time, obtain the c-AFM image through a series of scannings of mask border.The distance of the every 100 μ m of route that move along c-AFM probe is obtained 2 μ m * 2 μ m scan images.According to the number of obtained image, estimate that the distance of transition region 401 is approximately 200 μ m.Term used herein " transition region " is defined as the region at mask border place, when mask is placed in film when top, makes to be exposed on the film of photoflash lamp and forms corresponding conductive region, and wherein conducting film becomes non-conductive district from conduction region.
(E) according to the quantitatively characterizing of the conductivity of 4 point probe methods:
For the quantitatively characterizing of conductivity is provided to pattered region on the conducting film after exposure of flash lamp, we have used 4 detecting probe methods to record the scanning reading of every 0.5mm region sheet resistance (Rs).Fig. 5 is presented at the significant difference of the Rs reading between exposure (or unshielded) region and unexposed (or sheltering) region.Shadow region in Fig. 5 represents mask border or as transition region alleged in Fig. 4 401.When 4 probes move along mask border to unexposed (or sheltering) region from (or unshielded) region of exposing, Rs reading significantly increases (between minimum and high scale, having increased almost 1000 times).The conductivity that the so significant increase of Rs reading has disclosed film is carried out photocuring by exposure of flash lamp to exposed (unshielded) region and is significantly improved.
(F) Morphological Characterization of conducting film:
In the lower form of observing conducting film of scanning electron microscopy (SEM).Fig. 6 a shows to be coated on base material still mutually to pile up with the nano silver wire loosely by exposure of flash lamp.The insulated polyvinylpyrrolidone of these nano wires (PVP) residue around and contact point between described nano wire form high junction resistance.On the other hand, be coated on base material and the nano silver wire that is exposed to subsequently high-energy flashlamp of the present invention has produced more complete nano wire networking as shown in Figure 6 b.Nano wire after high-energy flashlamp exposure is fused together the structure that forms network sample.Interior heat between the nano wire that exposure of flash lamp produces greatly reduces junction resistance, makes (or unshielded) region exposing become and more conduct electricity than the film that uses conventional method.The PVP residue of the insulation in film is by high-energy flashlamp while photocuring of the present invention.Therefore, do not need in the present invention extra hot curing or etching step.
If needed, order that can be different and/or the difference in functionality of mutually side by side discussing herein.In addition, if needed, one or more above-mentioned function can be optional maybe can carry out combination.
Although described different aspect of the present invention in independent claims, other side of the present invention comprises other combinations from the feature of described embodiment and/or dependent claims and the feature of independent claims, and is not only the combination of clearly setting forth in the claims.
Although be also noted that in this article exemplary of the present invention has been described above, these explanations should not regarded determinate implication as.On the contrary, can carry out multiple variation and change and can not depart from scope of the present invention as defined by the appended claims.
Industrial applicibility
Method disclosed by the invention can be used for preparing the film of contact panel and other display, because can the cost-saving and time by the number of steps of using high-energy flashlamp to reduce as source generation high energy pulse.In reprocessing, avoid also can keeping the structure of nano wire and the conductivity of raising film by etched hot curing or chemosetting.It is also substantially invisible that the pattern being generated by method of the present invention in the situation that do not use has the material of the predetermined refractive index matching with film substrate.
Claims (22)
1. a method of preparing the transparent conducting film based on nano material, comprises
(a) the clean base material as conducting film carrier;
(b) provide the ink that contains nano material;
(c) ink that contains nano material described in coating on described base material is to form coated substrate;
(d) by physical mask, in one or more desired regions, shelter described coated substrate;
(e) described coated substrate is exposed to high-energy flashlamp source with coated substrate described in annealing and patterning, when described conducting film solidifies under described high-energy flashlamp source, forms the figuratum conducting film of tool thus.
2. the process of claim 1 wherein that described nano material is the nano wire based on silver-colored, described nano wire is linear, and draw ratio is greater than 150.
3. the process of claim 1 wherein that described nano material is the nano wire based on silver-colored, described nano wire is linear, and length is 10-15 μ m, and diameter is about 70nm.
4. the process of claim 1 wherein that described base material is PETG.
5. the process of claim 1 wherein that described cleaning comprises the following steps:
(a) with base material described in cleaning agent wiping;
(b) with base material described in deionized water rinsing;
(c) with base material described in acetone rinsing;
(d) at 70 ℃, be dried described base materials approximately 5 minutes;
(e) described base material is immersed in the isopropyl alcohol of boiling to approximately 10 minutes;
(f) described base material is rinsed with fresh isopropyl alcohol; With
(g) at 70 ℃, be dried described base materials approximately 5 minutes.
6. the ink that contains nano material described in the process of claim 1 wherein comprises a plurality of nano wires based on silver-colored and the solvent of about 90%v/v isopropyl alcohol/ethanol.
7. the method for claim 6, wherein said a plurality of nano wires based on silver-colored are dissolved in described solvent with concentration 10g/L.
8. the process of claim 1 wherein that described coating undertaken by having the apparatus for coating of Meyer rod.
9. the method for claim 8, wherein said Meyer rod is No. 4 Meyer rods.
10. described in the process of claim 1 wherein, be coated at approximately 34 ℃ and carry out.
The method of 11. claims 8, wherein said coating is further included under the help of syringe pump, and with the ink that contains nano material described in mobile interpolation of Meyer rod, adding speed is that 2-5ml/min or the size of adding speed and base material are proportional.
The method of 12. claims 11, the constant speed of 120cm per minute is controlled and is maintained at about in the movement of wherein said Meyer rod.
13. the process of claim 1 wherein that described coating is further included in physical mask is offered to described coated substrate before, at approximately 70 ℃, dry described coated substrate is approximately 5 minutes, then described coated substrate is divided into less piece.
14. methods claimed in claim 1, wherein said physical mask has the pattern corresponding to described desired regions, in described desired regions, when described physical mask is when horizontal level is between described high-energy flashlamp source and described coated substrate, the high energy optical pulses producing from described high-power lamps source is sheltered by described physical mask, it is non-conductive making described desired regions, and conduct electricity in other region of not sheltered by described physical mask.
15. methods claimed in claim 1, wherein said high-energy flashlamp source is to produce the photoflash lamp based on xenon of wavelength from 240nm to 1000nm light.
Method described in 16. claims 15, wherein said light has 370nm to the wavelength of 1000nm.
17. methods claimed in claim 1, wherein said coated substrate is exposed to about 1-120 second under described high-energy flashlamp source, and wherein average power density is about 10W/cm
2, pulsation rate is 2 pulses per second, or the pulse duration is about 0.52ms.
18. methods claimed in claim 1, wherein said high-energy flashlamp source produces peak power density at each impulse duration, and it is approximately 1000 times of average power density.
19. 1 kinds of nesa coatings of preparing according to the method for claim 1.
The nesa coating of 20. claims 19, wherein said film has the sheet resistance of about 15 Ω/ and surpasses 80% transmissivity.
The conducting film of 21. claims 19, wherein said film has the border around described desired regions of width approximately 200 μ m.
The nesa coating of 22. claims 19, nano material in other region of the described film of wherein not sheltered by described physical mask after described exposure forms the nanometer line network with the junction resistance reducing, and other polymer residue in same area is by photocuring, make described film have sightless pattern substantially, described pattern is corresponding to described desired regions and there is no masked region.
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| CN105164764A (en) * | 2013-04-26 | 2015-12-16 | 昭和电工株式会社 | Method for manufacturing electroconductive pattern and electroconductive pattern-formed substrate |
| CN107039098A (en) * | 2015-11-16 | 2017-08-11 | 三星电子株式会社 | The group of nano silver wire, its manufacture method including its electric conductor and electronic installation |
| CN109493734A (en) * | 2018-10-26 | 2019-03-19 | 深圳市华星光电半导体显示技术有限公司 | The production method of pixel electrode, display panel |
| CN109585057A (en) * | 2018-12-17 | 2019-04-05 | 太原理工大学 | A kind of flexible transparent conducting film and preparation method thereof based on layer assembly self-supporting film |
| CN111512401A (en) * | 2017-12-29 | 2020-08-07 | 爱泰德有限公司 | Method for manufacturing transparent electrode |
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